static headspace (hs) dynamic headspace spray-and-trap (st) spme membrane inlet

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Extraction Methods. Static Headspace (HS) Dynamic Headspace Spray-and-Trap (ST) SPME Membrane Inlet. Purge-and-Trap. Purge-and-Trap Method. Advantage : More sensitive than HS. Drawback : 1. Foaming and slowness of the purging step - PowerPoint PPT Presentation

TRANSCRIPT

Page 1: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet
Page 2: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet

Static Headspace (HS)

Dynamic Headspace

Spray-and-Trap (ST)

SPME

Membrane Inlet

Purge-and-Trap

Extraction Methods

Page 3: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet

Advantage : More sensitive than HS

Drawback : 1. Foaming and slowness

of the purging step

2. Large sample volume and

long purging time (10~30 min)

Purge-and-Trap Method

Page 4: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet

Experimental Aim

To construct an automated ST-

GC system for on-line

determination of dissolved VOCs

in water.

Page 5: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet

Carboxen 1000 Carboxen 1003

1/16”

Micro-sorbent Trap

Page 6: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet

Spray-and-Trap Device

Page 7: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet
Page 8: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet

Cleaning

Page 9: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet

Sampling

Page 10: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet

Mode A

Page 11: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet

Mode B

Page 12: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet

Injection

Page 13: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet
Page 14: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet

2. Amount of sample

3. Amount of extraction gas that is sampled.

Sensitivity of Mode A

1. Sprying condition

A. Size of droplet

B. Extraction gas flow rate

C. Design of nozzle

D. Introducing a limited amount of sample and extraction gas

Sensitivity of Mode A

Page 15: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet

Mode A VS. Mode B

A

Page 16: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet

Purge-and-Trap Device

Page 17: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet
Page 18: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet

Analytical conditions for ST and PT

Page 19: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet
Page 20: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet
Page 21: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet

Recoveries of ST methods

Recovery = PTresponse

STresponse

Page 22: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet

DL, R.S.D, and R2 for BTEX

Page 23: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet

Species

Chromatograms of ST-GC-ECD

1. CHCl3

2. CCl4

3. CH2Br2

4. CHCl=CCl2

5. CHBrCl2

6. CCl2=CCl2

Page 24: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet
Page 25: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet

Conclusion

An automated spray-and-trap device was built in the laboratory.

The studied ST method was validated in comparison with classic PT: recoveries precision, and linearity.

The ST method shows a fast response to abrupt changes in sample quality, which makes it suitable for on-site monitoring of a water body.

Page 26: Static Headspace (HS)  Dynamic Headspace  Spray-and-Trap (ST)  SPME  Membrane Inlet